CN106841065B - Ultraviolet-visible light-near infrared transmission and reflection spectrum measuring device and measuring method - Google Patents
Ultraviolet-visible light-near infrared transmission and reflection spectrum measuring device and measuring method Download PDFInfo
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Abstract
An ultraviolet-visible light-near infrared transmission reflection spectrum measuring device and a measuring method. The measuring device comprises a polychromatic light source, a grating monochromator, a diaphragm, a polaroid, a beam splitter, a reference light high-speed detector, a test light high-speed detector, an oscilloscope and a computer, and the measuring device has the advantages that: (1) the acquisition speed of the transflective spectrum is remarkably improved, and the rapid measurement of the transflective spectrum of the sample can be realized; (2) the measuring system has higher measuring precision, and the measuring error of the sample transmittance and reflectance is about 0.1-0.3%; (3) in the measuring process, mechanical parts in the grating monochromator always keep a uniform motion state, so that the testing system has high mechanical stability.
Description
Technical Field
The invention relates to measurement of a transmission-reflection spectrum, in particular to an ultraviolet-visible light-near infrared transmission-reflection spectrum measurement device and a measurement method.
Background
Ultraviolet-visible light-near infrared transmission and reflection spectrum measurement technology has obtained wide and important applications in scientific research fields such as physics, chemistry, biology, medicine, materials science, environmental science and the like, and in modern industrial production and management departments such as chemical industry, medicine, environmental detection, metallurgy and the like (see [1] Ni A, Huangmeizhen, Yuanbo, Zhaoyi, and sinus-crowing. ultraviolet-visible spectrophotometer development and present situation [ J ] modern scientific instruments, 2004,03:3-7+11 [2] Zhuying, and Huibone, Wuxiabo, Zhang Jun. ultraviolet-visible spectrophotometer and application [ J ] chemical intermediates, 2012,11:34-37 ]. At present, a measurement framework of a double-light-path photometry is commonly adopted for ultraviolet-visible light-near infrared transmission and reflection spectrums, as shown in fig. 1, and mainly comprises a polychromatic light source 1, a monochromator 2, a diaphragm 3, a polaroid 4, a beam splitter 5, a reference light detector 6, a sample to be measured 7, a test light detector 8, a data acquisition unit 9 and a computer 10. The polychromatic light emitted by the polychromatic light source passes through the monochromator to form monochromatic light required by measurement, the monochromatic light passes through the diaphragm and the polaroid to form linearly polarized light required by measurement, the linearly polarized light passes through the beam splitter to form a beam of measuring light and a beam of reference light, the reference light is collected by the reference light detector, the measuring light passes through a sample and is received by the test light detector, voltage signals output by the reference light detector and the test light detector are recorded by the data collector, and the computer is used for controlling the monochromator and performing data operation. Based on the current measurement system, the main measurement process of the sample transmission spectrum is as follows:
(1) measuring dark field intensity values of the reference light detector and the test light detector under the condition that the complex color light source is turned off;
(2) turning on the polychromatic light source, placing no sample in the light path, and irradiating the test light beam on the test light detector;
(3) setting the operating wavelength of the monochromator to lambda1Then, measuring the bright field intensity values of the reference light detector and the test light detector;
(4) setting the working wavelength of monochromator to lambda2,λ3……λnRespectively repeating the step (3) to obtain the bright field intensity values of the reference light detector and the test light detector under each wavelength;
(5) installing the sample to be tested in the test light beam, and setting the working wavelength of the monochromator as lambda1Then measuring the signal intensity values of the reference light detector and the test light detector;
(6) setting the working wavelength of monochromator to lambda2,λ3……λnRespectively repeating the step (5) to obtain signal intensity values of the reference light detector and the test light detector under each wavelength;
(7) respectively calculating the wavelength lambda according to the dark field intensity values of the reference light detector and the test light detector, and the bright field intensity value and the signal intensity value under each wavelength1,λ2,λ3……λnAnd the transmittance of the sample to be detected is measured, and the transmission spectrum of the sample to be detected is obtained.
The existing measuring device and measuring method can accurately complete the measurement of the sample transflective spectrum, and the measurement precision is about 0.1% -0.3%, but the following defects mainly exist:
(1) in the measurement process, the mechanical structure inside the monochromator needs to intermittently complete discontinuous intermittent motion (as shown in fig. 2, the emission wavelength of the monochromator is increased from 800nm to 810nm in a stepped manner within a certain time, and the emission wavelength of the monochromator is realized by moving an internal mechanical mechanism), the detector needs to perform intermittent data acquisition (as shown in fig. 3, a black dot represents the acquisition position of the detector), and the actions between the emission wavelength and the black dot are sequentially completed in time, so that the measurement speed of the sample transmission and reflection spectrum is slow, for example, in order to measure the transmission spectrum curve in the waveband range of 800nm to 1100nm, the time of about 3-5 minutes is often needed, and in the actual transmission spectrum measurement process, in order to observe the dynamic change condition of the sample transmission spectrum characteristic under the environmental factors of chemical reaction, temperature, humidity and the like, the transmission spectrum of a sample is required to be completed in a short time, and the currently generally adopted testing device and method are obviously insufficient; (2) in the existing measurement process of the sample transmission and reflection spectrum, mechanical components in the instrument need to keep an intermittent motion state, so that the mechanical stability of the test instrument is poor; (3) the measurement of the transmission and reflection spectrum of the sample is long in time consumption at present, and the working efficiency of a testing instrument is low, so that the testing requirement of a large batch of optical elements cannot be met.
The method for rapidly measuring the sample transmission and reflection spectrum based on the CCD is provided by patents (CN100451611C, CN1752739 and CN2837834Y) and research papers ([1] Tan Li, Liuyu Ling, Yu Feihong, development of a real-time measurement system of the spectral transmittance and reflectivity of an optical device [ J ] optical instrument, 2004,03:9-13 and [2] Liu Xuan Peak, Wangzhou, Zhang Baobaizi, a rapid spectral measurement and analysis system [ J ] photoelectric engineering, 2001,02: 27-31), but the method has the defects of low measurement precision and measurement error of about 5-8%. The Fourier TRANSFORM spectrometer (E.V. Loewenstein, "HISTORY AND CURRENT STATUS OFFOURER TRANSFORM SPECTROSCOPY," Applied Optics, vol.5, pp.845- +,1966.[2] jade-jade ], several core technical researches AND applications of the Fourier TRANSFORM infrared spectrometer [ D ]. Wuhan university, 2010 ]) can also realize the rapid measurement of the transmission AND reflection spectrum, but the main defects of the Fourier TRANSFORM infrared spectrometer are low in measurement precision AND the measurement error is about 2% -3%. Therefore, although multi-channel spectrometers and fourier transform spectrometers have been used to some extent in fast measurements, the disadvantage of low measurement accuracy makes them impractical for use in high accuracy, fast measurement environments.
Disclosure of Invention
The invention provides a measuring device and a measuring method of ultraviolet-visible light-near infrared transmission reflection spectrum, aiming at solving the problems in the existing measuring device and measuring method of ultraviolet-visible light-near infrared transmission reflection spectrum.
The technical solution of the invention is as follows:
the ultraviolet-visible light-near infrared transmission and reflection spectrum measuring device comprises a polychromatic light source, and a monochromator, a diaphragm, a polaroid and a beam splitter are sequentially arranged in the light beam output direction of the polychromatic light source.
The method for measuring the transmission spectrum of the sample to be measured by using the ultraviolet-visible light-near infrared transmission and reflection spectrum measuring device mainly comprises the following steps:
① no sample to be measured is placed in the light path, and the computer is used to control the exit wavelength of the monochromator from lambda1Increase to λ at uniform speednThe duration is t, the reference light high-speed detector (11) and the test light high-speed detector collect continuous light intensity signals, and the oscilloscope records the reference light high-speed detector and the test light high-speed detectorThe light intensity signal sequences collected by the detector are respectively recorded as
And
and inputting the data into the computer;
② the sample to be tested is installed in the light path between the beam splitter and the test light high-speed detector, and the computer controls the exit wavelength of the monochromator to be from lambda1Increase to λ at uniform speednThe duration is t, the reference light high-speed detector and the test light high-speed detector keep continuous light intensity signal acquisition, and the oscilloscope records light intensity signal sequences acquired by the reference light detector and the test light detector and respectively records the light intensity signal sequences as
And
and inputting the data into the computer;
thirdly, the computer calculates the transmittance sequence T (t) of the sample to be measured according to the following formula:
and fourthly, respectively calculating k and b according to the following formulas:
b＝λ1(1.7)
converting the abscissa t of the transmittance sequence T (t) into the wavelength lambda according to the following formula,
λ＝kt+b (1.8)
and obtaining the transmission spectrum T (lambda) of the sample (7) to be detected.
Compared with the existing measuring method of ultraviolet-visible light-near infrared transmission reflection spectrum, the measuring device and the measuring method of the invention simultaneously have the following advantages:
(1) the measuring speed is high. Because the scheme that the emergent wavelength of the monochromator continuously changes and the detector acquires the light intensity at a high speed is selected, the defect of low measuring speed of a common photometric method can be overcome, and the measurement of the transmission spectrum in the wave band range of 800-1100 nm can be completed within 2-5 seconds;
(2) the measurement precision is high. The measuring method is based on a double-light-path photometric method, and can achieve the same measuring precision (about 0.1-0.3%) of the photometric method;
(3) the mechanical stability is good. In the measuring process of the invention, the mechanical structure in the monochromator keeps a uniform motion state, and the test system has higher mechanical stability.
Drawings
FIG. 1 is a block diagram of a prior art UV-VIS-NIR transmission spectroscopy measurement architecture;
FIG. 2 is a graph of monochromator emission wavelength versus time during measurement in a prior art method;
FIG. 3 is a schematic diagram of the light intensity collection position during the measurement process of the prior art method;
FIG. 4 is a schematic view of an ultraviolet-visible-near infrared transmission spectrum measuring apparatus according to the present invention;
FIG. 5 is a graph of exit wavelength of monochromator versus time;
FIG. 6 is a schematic view of the light intensity collection position of the present invention;
fig. 7 is a schematic view of the ultraviolet-visible-near infrared reflectance spectrum measuring apparatus of the present invention.
Detailed Description
The invention is described in detail below with reference to the drawings and examples, but the scope of the invention should not be limited thereto.
The ultraviolet-visible light-near infrared transmission reflection spectrum measuring device mainly comprises a polychromatic light source 1, a monochromator 2, a diaphragm 3, a polaroid 4, a beam splitter 5, a sample 7 to be measured, a reference light high-speed detector 11, a test light high-speed detector 12, an oscilloscope 13 and a computer 10, wherein the monochromator 2, the diaphragm 3, the polaroid 4, the beam splitter 5, the sample 7 to be measured are arranged on the same plane of the reference light high-speed detector. The polychromatic light source 1 is used for providing polychromatic light sources for a measuring system, the monochromator 2 is used for converting the polychromatic light sources into monochromatic incident light beams, the diaphragm 3 is used for filtering stray light and adjusting the aperture of the incident light beams, the polaroid 4 is used for generating linearly polarized light required by measurement, the beam splitter 5 is used for forming a reference light beam and a test light beam, the reference light high-speed detector 11 is used for measuring the light intensity of the reference light beam at a high speed, the test light high-speed detector 12 is used for measuring the intensity of the test light beam at a high speed, the oscilloscope 13 is used for recording voltage signals collected by the reference light high-speed detector 11 and the test light high-speed detector 12, and the computer 12 is used for controlling the monochromator 2, controlling the oscilloscope 13 and.
The working principle is as follows:
in the ultraviolet-visible light-near infrared transmission and reflection spectrum measuring device shown in fig. 4, polychromatic light emitted by a polychromatic light source 1 is sequentially transmitted through a monochromator 2, a diaphragm 3, a polarizing plate 4 and a beam splitter 5, then a beam of reference light and a beam of test light are formed, the light intensity of the reference light is collected by a reference light high-speed detector 11, and the test light is collected by a test light high-speed detector 12 after passing through a sample 7 to be measured.
During measurement, the monochromator and oscilloscope are controlled by a computer to make the emergent wavelength of the monochromator from lambda1Increase to λ at uniform speedn(as shown in fig. 5, the emission wavelength of the monochromator is continuously increased from 800nm to 810nm within a certain time), and meanwhile, the reference light high-speed detector and the test light high-speed detector keep continuous light intensity acquisition (as shown in fig. 6, black dots represent the acquisition positions of the high-speed detector), the oscilloscope is used for recording analog voltage signals acquired by the reference light high-speed detector and the test light high-speed detector, and the computer is used for data processing and operation.
Based on the measurement device of ultraviolet-visible light-near infrared transmission reflection spectrum shown in fig. 4, the rapid measurement method of ultraviolet-visible light-near infrared transmission reflection spectrum of the invention mainly comprises the following steps:
① the exit wavelength of the monochromator is made to be from lambda by a computer without placing a sample in the light path1Increase to λ at uniform speednDuration t, while making the ginsengThe test light high-speed detector and the test light high-speed detector collect continuous light intensity signals, and an oscilloscope records light intensity signal sequences collected by the reference light high-speed detector and the test light high-speed detector respectively as
And
② A sample to be tested is arranged in the light path between the beam splitter and the high-speed detector of test light, and the computer is used to make the exit wavelength of monochromator from lambda1Increase to λ at uniform speednKeeping the reference light high-speed detector and the test light high-speed detector to continuously acquire light intensity signals with duration time t, and recording the light intensity signal sequences acquired by the reference light detector and the test light detector by using an oscilloscope respectively as
And
③ light intensity sequences obtained according to steps ① and ②
And
calculating the transmittance sequence T (t) of the sample to be measured by using a computer according to the following formula:
and fourthly, respectively calculating k and b according to the following formulas:
b＝λ1(1.11)
and fifthly, converting the abscissa T of the transmittance sequence T (T) into the wavelength lambda according to the following formula to obtain the transmission spectrum T (lambda) of the sample to be measured.
λ＝kt+b (1.12)
Example 1:
FIG. 4 is a structural diagram of the measurement device of the ultraviolet-visible light-near infrared transmission spectrum of the present invention, a light source 1 adopts a FemtoPower FP1060-20 supercontinuum fiber laser, a monochromator 2 adopts a Photon series grating monochromator, a diaphragm 3 adopts an ID20 extension rod of Thorlabs company to install an iris diaphragm, a polarizer 4 adopts an LPVIS050-MP2 linear polarizer of Thorlabs company, a beam splitter 5 adopts a thin film beam splitter installed in a CM1-BP145B2 cage cube of Thorlabs company, a sample 7 is a transmission sample, a reference light high speed detector 11 and a test light high speed detector 12 both adopt a 1811 series high speed photodetector GS with a Newport bandwidth of 150MHZ, and an oscilloscope 13 adopts a DPO7054C series oscilloscope with a Tektronix bandwidth of 500MHZ and a sampling rate of 5/s.
Example 2:
FIG. 7 is a structural diagram of the ultraviolet-visible light-near infrared reflection spectrum measuring device of the present invention, a light source 1 adopts a FemtoPower FP1060-20 supercontinuum fiber laser, a monochromator 2 adopts a Photon series grating monochromator, a diaphragm 3 adopts an ID20 extension rod of Thorlabs company to install an iris diaphragm, a polarizer 4 adopts an LPVIS050-MP2 linear polarizer of Thorlabs company, a beam splitter 5 adopts a thin film beam splitter installed in a CM1-BP145B2 cage cube of Thorlabs company, a sample 14 is a reflection sample, a reference light high speed detector 11 and a test light high speed detector 12 both adopt a 1811 series high speed photodetector with a Newport bandwidth of 150MHZ, and an oscilloscope GS 13 adopts a DPO70 7054C series oscilloscope with a Tektronix bandwidth of 500MHZ and a sampling rate of 5/s.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. An ultraviolet-visible light-near infrared transmission and reflection spectrum measuring device comprises a polychromatic light source (1), wherein a monochromator (2), a diaphragm (3), a polaroid (4) and a beam splitter (5) are sequentially arranged in the beam output direction of the polychromatic light source (1), the ultraviolet-visible light-near infrared transmission and reflection spectrum measuring device is characterized in that a reference light high-speed detector (11) is arranged in the reference light emergent direction of the beam splitter (5), a sample to be measured (7) and a test light high-speed detector (12) are sequentially arranged in the test light emergent direction of the beam splitter (5), the output end of the reference light high-speed detector (11) is connected with the first input end of an oscilloscope (13), the output end of the test light high-speed detector (12) is connected with the second input end of the oscilloscope (13), the output end of the oscilloscope (13) is connected with the input end of a computer (10), the output end of the computer (10) is connected with the control end of the monochromator (2), and the emergent wavelength of the monochromator (2) is continuously changed.
2. The method for measuring the transmission spectrum of a sample (7) to be measured by using the ultraviolet-visible light-near infrared transreflective spectrometry apparatus as claimed in claim 1, mainly comprising the steps of:
① No sample (7) to be measured is placed in the light path, the computer (10) is used to control the outgoing wavelength of the monochromator (2) from lambda1Increase to λ at uniform speednThe duration is t, the reference light high-speed detector (11) and the test light high-speed detector (12) collect continuous light intensity signals, and the oscilloscope (13) records light intensity signal sequences collected by the reference light high-speed detector (11) and the test light high-speed detector (12) and respectively records the light intensity signal sequences as t
And
and input into said computer (10);
② a sample (7) to be tested is arranged in the light path between the beam splitter (5) and the test light high-speed detector (12), and the computer (10) controls the monochromatic lightThe exit wavelength of the device (2) is from lambda1Increase to λ at uniform speednThe duration is t, the reference light high-speed detector (11) and the test light high-speed detector (12) keep continuous light intensity signal acquisition, and the oscilloscope (13) records light intensity signal sequences acquired by the reference light detector (11) and the test light detector (12) and respectively records the light intensity signal sequences as t
And
and input into said computer (10);
thirdly, the computer (10) calculates the transmittance sequence T (t) of the sample (7) to be measured according to the following formula:
and fourthly, respectively calculating k and b according to the following formulas:
b＝λ1(1.3)
converting the abscissa t of the transmittance sequence T (t) into the wavelength lambda according to the following formula,
λ＝kt+b (1.4)
and obtaining the transmission spectrum T (lambda) of the sample (7) to be detected.
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